CN107555428A - A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite - Google Patents
A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite Download PDFInfo
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Abstract
The present invention relates to micro crystal graphite purification technique field, discloses a kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite.The micro crystal graphite secondary pickling method of purification includes the processing of S1. raw ores；S2. the acidleach purification of two times.Raw ore of the present invention by one of technique of flotation, is then purified using the two step acid-hatchings of young eggs to micro crystal graphite first, and fixed carbon content can reach more than 99.9%, significantly reduce the usage amount of hydrofluoric acid, has the advantages of efficiency high, energy consumption are low, and refining effect is good.It is limited to solve prior art chemical purification effect, the problem of fixed carbon content is unable to reach more than 99.9%, and high temperature method cost is too high.
Description
Technical field
The present invention relates to micro crystal graphite purification technique field, is purified more particularly, to a kind of micro crystal graphite secondary pickling
Method and its high-purity micro crystal graphite.
Background technology
Graphite is a kind of high energy crystal carbon material, because of its unique structure and conduction, heat conduction, lubrication, high temperature resistant, chemically
Can be stable the features such as, be widely used in metallurgy, machinery, environmental protection, chemical industry, fire resisting, new energy, nuclear energy, electronics, medicine, military project and
The fields such as Aero-Space.
Native graphite shaping geological conditions in China is good, widely distributed, aboundresources, quality are good, and reserves and yield all occupy generation
Boundary is the first, is one of the Dominant Mineral Resources in China.Native graphite can be divided into Scaly graphite and microcrystalline according to the difference of crystallization degree
The class of graphite two, wherein Chenzhou aphanitic graphite account for 74.7% or so of national gross reserves, and the aphanitic graphite quality is preferable,
Fixed carbon content is high.
But for a long time, people mostly pay attention to the exploitation and processing of Scaly graphite, ignore and occupy a greater part of reserves
The utilization of microcrystalline graphite, the problem of its deep process technology is horizontal and deep processing ability is relatively low, are not solved effectively for a long time
Certainly.At present mainly based on raw ore and rough-wrought product application, resource is not fully utilized, or even blindly exports, and causes ore deposit
Produce a large amount of losses and waste of resource.Therefore, the chemical purification research work of microcrystalline graphite, developing low-cost high-carbon stone are carried out
Black production technology, has important practical significance.
The purification of microcrystalline graphite at present mostly be use for reference Scaly graphite technology, common method of purification include floatation,
High temperature method, alkali acid system, hydrogen fluoride, chlorinating roasting etc., floatation are used for the preliminary purification of Scaly graphite, graphite products product
Position is not high, and the rate of recovery is very low, the method for the non-chemical purification graphite of alkali acid system, hydrogen fluoride, chlorinating roasting, wherein, alkali
Acid system purifies the shortcomings that graphite and is to need high-temperature calcination, and energy expenditure is big, and the reaction time length purified, and the method pair sets
Standby corrosion is more serious, and the graphite purity obtained by the method does not reach 99.9%, although high temperature method refining effect
Preferably, but its cost is too high, capital invested needed for industrialization is huge, and hydrogen fluoride purification graphite efficiency high, energy consumption are low, but hydrogen
The dosage of fluoric acid is huge and has severe toxicity and severe corrosive, causes production equipment and environmentally friendly cost higher.
The content of the invention
The technical problems to be solved of the present invention are, fixed carbon content limited for prior art chemical purification effect
More than 99.9% is unable to reach, and high temperature method cost is too high, further to improve graphite purity and reducing the dosage of hydrofluoric acid,
A kind of micro crystal graphite secondary pickling method of purification is provided.
The present invention also provides a kind of high-purity micro crystal graphite being prepared using the above method, fixed carbon content be for
More than 99.99%.
The purpose of the present invention is achieved by the following technical programs：
A kind of micro crystal graphite secondary pickling method of purification is provided, comprised the following steps：
S1. raw ore is handled：It is 75~80% micro crystal graphite crushing raw ores by fixed carbon content, then to micro crystal graphite raw ore
Depth ore grinding is carried out, it is -0.074mm level materials to obtain fineness by ore grinding, is -0.074mm level material contents to mog
The primary sample for accounting for 90% carries out flotation, afterwards drying, magnetic separation, and it is 85~90% micro crystal graphites to be fixed carbon content；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 and mixed acid are mixed, the mixed acid is HF and H2SO4's
Mixed acid, the concentration of the HF is 5~10%, the H2SO4Concentration be 20~40%, mixed acid and graphite liquid-solid ratio be 2~
3.5:1, normal pressure acidleach is then carried out under conditions of 50~80 DEG C of temperature, 1~3h of reaction time, leached mud, which is washed to pH value, is
Neutrality, filtering, dry, it is more than 98% micro crystal graphite to be fixed carbon content；
S22. secondary pickling：The obtained micro crystal graphites of step S21 and mixed acid are mixed, the mixed acid is HF and H2SO4
Mixed acid, the concentration of the HF is 2~4%, the H2SO4Concentration be 10~30%, mixed acid and graphite liquid-solid ratio are 2
~4:1, stir and be ultrasonically treated, the time is 10~30min, is subsequently placed on magnetic stirring apparatus, reaction temperature 60~
90 DEG C, 1~3h of reaction time, pH value is then washed to as neutrality, filtering, is dried, is fixed carbon content as more than 99.9%
High-purity micro crystal graphite.
The present invention carries out preliminary treatment using one of floatation process to raw ore first, graphite purity is improved, after reduction
The dosage of continuous hydrofluoric acid, using two step acidleach, in the graphite after being purified to an acidleach, residual impurity, which uses, is ultrasonically treated, so as to
The usage amount of hydrofluoric acid is reduced, is fixed high-purity micro crystal graphite that carbon content is more than 99.99%.
Preferably, micro crystal graphite raw ore described in step S1 is Shandong pool micro crystal graphite, the moisture of Shandong pool micro crystal graphite
For 2.4%, volatilization is divided into 2.99%, and ash content is that 18.37% carbon content is 78.64%.
Preferably, flotation described in step S1 uses four selected once purging selection flows of one roughing.
Preferably, the concentration of HF described in step S21 is 7%, H2SO4Concentration be 30%, liquid-solid ratio 3.5:1.
Preferably, the concentration of HF described in step S22 is 3%, the H2SO4Concentration be 20%, liquid-solid ratio 3:1.
Preferably, ultrasonic time described in step S22 is 15min.
Preferably, drying described in step S21 is to dry 2~3h in the case where temperature is 80~150 DEG C.
Preferably, drying described in step S22 is to dry 2~3h in the case where temperature is 80~150 DEG C.
The present invention also provides a kind of high-purity micro crystal graphite being prepared using the above method, and fixed carbon content is 99.9%
More than.
Compared with prior art, the beneficial effects of the invention are as follows：
Raw ore of the present invention by one of technique of flotation, is then purified using the two step acid-hatchings of young eggs to micro crystal graphite first,
Fixed carbon content can reach more than 99.9%, significantly reduce the usage amount of hydrofluoric acid, have efficiency high, energy consumption low, purification is imitated
The advantages of fruit is good.
The present invention carries out crystallite stone mill raw ore and is crushed and ground first, coordinates the one roughing four times selected one of flotation
It is secondary to scan flow, the purity of raw ore is at utmost improved (if fixed carbon content is gone back for 90% micro crystal graphite by physical method
Its grade is set to be further enhanced, floatation is all than relatively difficult to achieve in technology or economically) while reduce
Micro crystal graphite particle diameter, increase the specific surface area of micro crystal graphite, be advantageous to reduce in follow-up acidleach purification subsequent purification energy consumption and
Cost.
The present invention is purified using the two step acid-hatchings of young eggs to micro crystal graphite, wherein for the first time using graphite after acid-hatching of young eggs purification
In impurity volume significantly reduce, metamorphosis is larger, but still exists in granular form, reason be with reaction carry out,
Impurity particle ecto-entad gradually dissolves, and reaction difficulty gradually increases, and these precipitations are covered in undissolved impurity particle
Surface, the further progress of reaction is hindered, now continue the concentration effect and unobvious of increase acid, in addition, these precipitations are originally
It is difficult to be removed in the washing and filtering stage, the present invention creatively adds ultrasonication so that after acidleach purification
Micro crystal graphite is additionally separated with impurity, and the mechanical crushing effect and cavitation in ultrasonic procedure can be by micro crystal graphites
Particle crushes, and makes to be wrapped in the partial impurities in aggregate and participates in reaction, accelerates the reaction rate of impurity and acid, therefore, the
Secondary pickling purification only needs minimal amount of acid to can obtain high-purity micro crystal graphite, significantly reduces purification energy consumption and cost.
Brief description of the drawings
Fig. 1 flotation flowsheet figures
Embodiment
The present invention is further illustrated with reference to specific embodiment.Following examples are only illustrative examples, not structure
Into inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and covered by the content of the invention is implemented.It is unless special
Do not mentionlet alone bright, the present invention reagent, compound and the equipment that use is the art conventional reagent, compound and equipment.
Embodiment 1
The present embodiment provides a kind of micro crystal graphite secondary pickling method of purification, comprises the following steps：
S1. raw ore is handled：By Shandong pool micro crystal graphite crushing raw ore, depth ore grinding then is carried out to micro crystal graphite raw ore, led to
It is -0.074mm level materials to cross ore grinding and obtain fineness, is that -0.074mm level material contents account for 90% primary sample and entered to mog
Row flotation, as shown in figure 1, using drying, magnetic separation after four selected once purging selection flows of one roughing, it is fixed carbon content
For 90% micro crystal graphite；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content
18.37% carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 and mixed acid are mixed, the mixed acid is HF and H2SO4's
Mixed acid, the concentration of the HF is 5%, the H2SO4Concentration be 20%, mixed acid and graphite liquid-solid ratio are 2:1, Ran Hou
Normal pressure acidleach is carried out under conditions of temperature 50 C, reaction time 1h, it is neutrality that leached mud, which is washed to pH value, filters, is in temperature
2~3h is dried at 80~150 DEG C, is fixed the micro crystal graphite that carbon content is 98.07%；
S22. secondary pickling：The obtained micro crystal graphites of step S21 and mixed acid are mixed, the mixed acid is HF and H2SO4
Mixed acid, the concentration of the HF is 2%, the H2SO4Concentration be 10%, mixed acid and graphite liquid-solid ratio are 2:1, stirring
Uniformly it is ultrasonically treated, the time is 10~30min, is subsequently placed on magnetic stirring apparatus, 60 DEG C of reaction temperature, reaction time
1h, pH value is then washed to as neutrality, filtering, dry 2~3h at being 80~150 DEG C in temperature, being fixed carbon content is
99.91% high-purity micro crystal graphite.
Embodiment 2
The present embodiment provides a kind of micro crystal graphite secondary pickling method of purification, comprises the following steps：
S1. raw ore is handled：By Shandong pool micro crystal graphite crushing raw ore, depth ore grinding then is carried out to micro crystal graphite raw ore, led to
It is -0.074mm level materials to cross ore grinding and obtain fineness, is that -0.074mm level material contents account for 90% primary sample and entered to mog
Row flotation, as shown in figure 1, using drying, magnetic separation after four selected once purging selection flows of one roughing, it is fixed carbon content
For 90% micro crystal graphite；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content
18.37% carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 and mixed acid are mixed, the mixed acid is HF and H2SO4's
Mixed acid, the concentration of the HF is 7%, the H2SO4Concentration be 30%, mixed acid and graphite liquid-solid ratio are 3.5:1, then
Normal pressure acidleach is carried out under conditions of 80 DEG C of temperature, reaction time 3h, it is neutrality that leached mud, which is washed to pH value, is filtered, in temperature
To dry 2~3h at 80~150 DEG C, the micro crystal graphite that carbon content is 98.82% is fixed；
S22. secondary pickling：The obtained micro crystal graphites of step S21 and mixed acid are mixed, the mixed acid is HF and H2SO4
Mixed acid, the concentration of the HF is 3%, the H2SO4Concentration be 20%, mixed acid and graphite liquid-solid ratio are 3:1, stirring
Uniformly it is ultrasonically treated, time 15min, is subsequently placed on magnetic stirring apparatus, 90 DEG C of reaction temperature, reaction time 3h, so
After be washed to pH value as neutrality, filtering, dry 2~3h at being 80~150 DEG C in temperature, be fixed carbon content as 99.98%
High-purity micro crystal graphite.
Embodiment 3
The present embodiment provides a kind of micro crystal graphite secondary pickling method of purification, comprises the following steps：
S1. raw ore is handled：By Shandong pool micro crystal graphite crushing raw ore, depth ore grinding then is carried out to micro crystal graphite raw ore, led to
It is -0.074mm level materials to cross ore grinding and obtain fineness, is that -0.074mm level material contents account for 90% primary sample and entered to mog
Row flotation, as shown in figure 1, using drying, magnetic separation after four selected once purging selection flows of one roughing, it is fixed carbon content
For 90% micro crystal graphite；
The raw ore material performance of Shandong pool micro crystal graphite described in step S1 is as follows：Moisture 2.4%, volatile matter 2.99%, ash content
18.37% carbon content 78.64%；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 and mixed acid are mixed, the mixed acid is HF and H2SO4's
Mixed acid, the concentration of the HF is 10%, the H2SO4Concentration be 40%, mixed acid and graphite liquid-solid ratio are 3.5:1, then
Normal pressure acidleach is carried out under conditions of 80 DEG C of temperature, reaction time 3h, it is neutrality that leached mud, which is washed to pH value, is filtered, in temperature
To dry 2~3h at 80~150 DEG C, the micro crystal graphite that carbon content is 98.86% is fixed；
S22. secondary pickling：The obtained micro crystal graphites of step S21 and mixed acid are mixed, the mixed acid is HF and H2SO4
Mixed acid, the concentration of the HF is 4%, the H2SO4Concentration be 30%, mixed acid and graphite liquid-solid ratio are 4:1, stirring
Uniformly it is ultrasonically treated, time 30min, is subsequently placed on magnetic stirring apparatus, 90 DEG C of reaction temperature, reaction time 3h, so
After be washed to pH value as neutrality, filtering, dry 2~3h at being 80~150 DEG C in temperature, be fixed carbon content as 99.98%
High-purity micro crystal graphite.
Comparative example 1
This comparative example is substantially the same manner as Example 1, and difference is, does not use supersound process in step S22.
This comparative example does not use supersound process under the mixed acid of low concentration, and obtained micro crystal graphite fixes carbon content and is
98.23%, illustrate in the case of not using supersound process, secondary pickling is substantially limited to further refining effect, and lifting is not
Substantially.
Comparative example 2
This comparative example is essentially identical with comparative example, and difference is, progressively increases the concentration of mixed acid in step S22,
It is specific as shown in table 1.
Table 1
| Liquid-solid ratio | HF concentration (%) | Sulfuric acid concentration (%) | Fixed carbon content |
| 2：1 | 5 | 10 | 99.55 |
| 2：1 | 10 | 20 | 99.68 |
| 2：1 | 20 | 30 | 99.74 |
| 2：1 | 30 | 40 | 99.74 |
It can be seen from table 1, when HF concentration reaches 20%, when sulfuric acid concentration reaches 30%, now fixed carbon content has reached
To the limit, lifting that can not be further, therefore the dosage of hydrofluoric acid is not only greatly reduced using the present invention, reduce purification
Cost and energy consumption, and fixed carbon content can be promoted to more than 99.99%.
Claims (10)
1. a kind of micro crystal graphite secondary pickling method of purification, it is characterised in that comprise the following steps：
S1. raw ore is handled：It is 75~80% micro crystal graphite crushing raw ores by fixed carbon content, then micro crystal graphite raw ore is carried out
Depth ore grinding, it is -0.074mm level materials to obtain fineness by ore grinding, is that -0.074mm level material contents account for 90% to mog
Primary sample carry out flotation, afterwards drying, magnetic separation, it is 85~90% micro crystal graphites to be fixed carbon content；
S2. acidleach purifies：
S21. an acidleach：Micro crystal graphite obtained by step S1 and mixed acid are mixed, the mixed acid is HF and H2SO4Mixing
Acid, the concentration of the HF is 5~10%, the H2SO4Concentration be 20~40%, mixed acid and graphite liquid-solid ratio are 2~3.5:1,
Then normal pressure acidleach is carried out under conditions of 50~80 DEG C of temperature, 1~3h of reaction time, it is neutrality that leached mud, which is washed to pH value,
Filtering, dry, it is more than 98% micro crystal graphite to be fixed carbon content；
S22. secondary pickling：The obtained micro crystal graphites of step S21 and mixed acid are mixed, the mixed acid is HF and H2SO4It is mixed
Acid is closed, the concentration of the HF is 2~4%, the H2SO4Concentration be 10~30%, mixed acid and graphite liquid-solid ratio are 2~4:1,
Stir and be ultrasonically treated, the time is 10~30min, is subsequently placed on magnetic stirring apparatus, 60~90 DEG C of reaction temperature, anti-
1~3h between seasonable, it is neutrality to be washed out to pH value, filtering, is dried, be fixed carbon content be more than 99.9% it is high-purity micro-
Spar ink.
2. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that microlite described in step S1
Black raw ore is Shandong pool micro crystal graphite.
3. micro crystal graphite secondary pickling method of purification according to claim 2, it is characterised in that Shandong pool micro crystal graphite
Moisture is 2.4%, and volatilization is divided into 2.99%, and ash content is that 18.37% carbon content is 78.64%.
4. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that flotation is adopted described in step S1
With four selected once purging selection flows of one roughing.
5. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that HF described in step S21
Concentration is 7%, H2SO4Concentration be 30%, liquid-solid ratio 3.5:1.
6. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that HF described in step S22
Concentration is 3%, the H2SO4Concentration be 20%, liquid-solid ratio 3:1.
7. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that ultrasonic described in step S22
Time is 15min.
8. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that dried described in step S21
It is to dry 2 ~ 3h in the case where temperature is 80 ~ 150 DEG C.
9. micro crystal graphite secondary pickling method of purification according to claim 1, it is characterised in that dried described in step S22
It is to dry 2 ~ 3h in the case where temperature is 80 ~ 150 DEG C.
10. the high-purity crystallite being prepared according to micro crystal graphite secondary pickling method of purification described in claim 1~6 any one
Graphite, it is characterised in that high-purity micro crystal graphite carbon content is more than 99.9%.
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Cited By (12)
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| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
| CN110156006A (en) * | 2019-07-10 | 2019-08-23 | 青岛洛唯新材料有限公司 | A kind of purification process technique of graphite |
| CN110217787A (en) * | 2019-05-27 | 2019-09-10 | 内蒙古瑞盛新能源有限公司 | A method of micro crystal graphite is purified using industrial waste acid |
| CN110294473A (en) * | 2019-06-06 | 2019-10-01 | 湖南中科星城石墨有限公司 | The preparation process of organic acid catalysis purification micro crystal graphite |
| CN111751311A (en) * | 2020-07-03 | 2020-10-09 | 中南大学 | Preparation method of graphite material for oxygen-nitrogen-hydrogen analyzer |
| CN112520733A (en) * | 2020-12-01 | 2021-03-19 | 萝北瑞喆烯碳新材料有限公司 | Chemical purification method for graphite |
| CN114455579A (en) * | 2022-03-04 | 2022-05-10 | 杨德俊 | Method for purifying natural graphite |
| CN115321530A (en) * | 2022-07-05 | 2022-11-11 | 北京科技大学 | High-purity crystalline graphite and preparation method thereof |
| CN115557495A (en) * | 2021-07-01 | 2023-01-03 | 中国科学院过程工程研究所 | Low-fluorine purification method for natural graphite spherical tailings |
| CN115716645A (en) * | 2022-12-09 | 2023-02-28 | 武汉理工大学 | Purification method of spherical graphite mixed acid leaching-ultrasonic water washing |
| CN116902975A (en) * | 2023-09-12 | 2023-10-20 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
| CN117819541A (en) * | 2024-03-04 | 2024-04-05 | 矿冶科技集团有限公司 | Method for purifying graphite by high-temperature drying-free raw materials and simple acid-base method |
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| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
| CN110217787A (en) * | 2019-05-27 | 2019-09-10 | 内蒙古瑞盛新能源有限公司 | A method of micro crystal graphite is purified using industrial waste acid |
| CN110294473A (en) * | 2019-06-06 | 2019-10-01 | 湖南中科星城石墨有限公司 | The preparation process of organic acid catalysis purification micro crystal graphite |
| CN110294473B (en) * | 2019-06-06 | 2021-03-05 | 湖南中科星城石墨有限公司 | Preparation process for purifying microcrystalline graphite by organic acid catalysis |
| CN110156006A (en) * | 2019-07-10 | 2019-08-23 | 青岛洛唯新材料有限公司 | A kind of purification process technique of graphite |
| CN111751311A (en) * | 2020-07-03 | 2020-10-09 | 中南大学 | Preparation method of graphite material for oxygen-nitrogen-hydrogen analyzer |
| CN112520733A (en) * | 2020-12-01 | 2021-03-19 | 萝北瑞喆烯碳新材料有限公司 | Chemical purification method for graphite |
| CN115557495A (en) * | 2021-07-01 | 2023-01-03 | 中国科学院过程工程研究所 | Low-fluorine purification method for natural graphite spherical tailings |
| CN114455579A (en) * | 2022-03-04 | 2022-05-10 | 杨德俊 | Method for purifying natural graphite |
| CN115321530A (en) * | 2022-07-05 | 2022-11-11 | 北京科技大学 | High-purity crystalline graphite and preparation method thereof |
| CN115716645A (en) * | 2022-12-09 | 2023-02-28 | 武汉理工大学 | Purification method of spherical graphite mixed acid leaching-ultrasonic water washing |
| CN116902975A (en) * | 2023-09-12 | 2023-10-20 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
| CN116902975B (en) * | 2023-09-12 | 2024-03-12 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
| CN117819541A (en) * | 2024-03-04 | 2024-04-05 | 矿冶科技集团有限公司 | Method for purifying graphite by high-temperature drying-free raw materials and simple acid-base method |
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Application publication date: 20180109 |